# Electronic Supplementary Material (ESI) for Dalton Transactions
# This journal is © The Royal Society of Chemistry 2013


#######################################################################
#
#                 Cambridge Crystallographic Data Centre
#                                CCDC 
# 
#######################################################################
# 
#  This CIF contains data from an original supplementary publication 
#  deposited with the CCDC, and may include chemical, crystal,   
#  experimental, refinement, atomic coordinates, 
#  anisotropic displacement parameters and molecular geometry data,
#  as required by the journal to which it was submitted. 
# 
#  This CIF is provided on the understanding that it is used for bona
#  fide research purposes only. It may contain copyright material 
#  of the CCDC or of third parties, and may not be copied or further 
#  disseminated in any form, whether machine-readable or not,  
#  except for the purpose of generating routine backup copies 
#  on your local computer system.
# 
#  For further information on the CCDC, data deposition and 
#  data retrieval see:
#                         www.ccdc.cam.ac.uk 
#
#  Bona fide researchers may freely download Mercury and enCIFer
#  from this site to visualise CIF-encoded structures and 
#  to carry out CIF format checking respectively. 
#
####################################################################### 

data_1
_database_code_depnum_ccdc_archive 'CCDC 912234'
#TrackingRef 'Compound-1.CIF'
_vrf_PLAT601_1                   
;
PROBLEM: Structure Contains Solvent Accessible VOIDS
RESPONSE: The accessible solvent void in the crystal
structure indicates that some more water molecules should
exist in the structure, but cannot be found from the weak
residual electron peaks. Based on the TG analyses,
another 23 water molecules were included in the sum formula.
;
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C20 H194 Cu5 Ge8 N20 Na10 Nb32 O163'
_chemical_formula_weight         7425.39
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Ge Ge 0.1547 1.8001 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           Orthorhombic
_symmetry_space_group_name_H-M   Immm
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x, -y, z'
'-x, y, -z'
'x, -y, -z'
'x+1/2, y+1/2, z+1/2'
'-x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, -z+1/2'
'-x, -y, -z'
'x, y, -z'
'x, -y, z'
'-x, y, z'
'-x+1/2, -y+1/2, -z+1/2'
'x+1/2, y+1/2, -z+1/2'
'x+1/2, -y+1/2, z+1/2'
'-x+1/2, y+1/2, z+1/2'
_cell_length_a                   15.104(3)
_cell_length_b                   25.920(5)
_cell_length_c                   30.280(6)
_cell_angle_alpha                90.00
_cell_angle_beta                 90.00
_cell_angle_gamma                90.00
_cell_volume                     11855(4)
_cell_formula_units_Z            2
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    7268
_cell_measurement_theta_min      3.01
_cell_measurement_theta_max      27.48
_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.27
_exptl_crystal_size_mid          0.14
_exptl_crystal_size_min          0.09
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.080
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             7162
_exptl_absorpt_coefficient_mu    3.028
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.4952
_exptl_absorpt_correction_T_max  0.7722
_exptl_absorpt_process_details   'ABSCOR by T.Higashi 8 March, 1995'
_exptl_special_details           
;
In the refinement, all positions of Na ions and solvent water
molecules were firstly confirmed based on the distance references
(Na/Na > 3.0 ?, O/O > 2.5 ?). Then, their site occupancies were
determined as follows: For Na cations, only Na1 and Na2 is well
confirmed and fully occupied. The site occupancies of Na3, Na4 and
Na5 were calculated by fixing their Ueq values, which are 1.2
times larger than the one of Na2. The final calculated values are
ca. 0.10, 0.16 and 0.24. Thus, the site occupancies of Na3 CNa5
were determined. Following the same method, the site occupancies
of disordered solvent water molecules were also confirmed. About
18 lattice water molecules were found from the Fourier maps,
however, there are still a very large accessible solvent voids
in the crystal structure, indicating that some more water molecules
should exist in the structure, but cannot be found from the weak
residual electron peaks. Based on the TG analyses, another
23 water molecules were included in the sum formula based on
the TG analyses. The restraint command 'isor' was employed
to restrain na3, na5, c1, c2, o1w and o2w atoms so as to
avoid the ADP and NPD problems on them. This command led to
a restraint number 37.
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       Oscillation
_diffrn_detector_area_resol_mean 0.01
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        none
_diffrn_reflns_number            51755
_diffrn_reflns_av_R_equivalents  0.0855
_diffrn_reflns_av_unetI/netI     0.0546
_diffrn_reflns_limit_h_min       -19
_diffrn_reflns_limit_h_max       19
_diffrn_reflns_limit_k_min       -33
_diffrn_reflns_limit_k_max       33
_diffrn_reflns_limit_l_min       -39
_diffrn_reflns_limit_l_max       36
_diffrn_reflns_theta_min         3.01
_diffrn_reflns_theta_max         27.48
_reflns_number_total             7268
_reflns_number_gt                5009
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       auto
_computing_cell_refinement       auto
_computing_data_reduction        auto
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.1030P)^2^+227.7623P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         7268
_refine_ls_number_parameters     310
_refine_ls_number_restraints     37
_refine_ls_R_factor_all          0.0976
_refine_ls_R_factor_gt           0.0665
_refine_ls_wR_factor_ref         0.2095
_refine_ls_wR_factor_gt          0.1913
_refine_ls_goodness_of_fit_ref   1.053
_refine_ls_restrained_S_all      1.054
_refine_ls_shift/su_max          0.012
_refine_ls_shift/su_mean         0.001
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.0000 0.21563(5) 0.16716(4) 0.0322(3) Uani 1 2 d S . .
Nb2 Nb 0.12526(8) 0.32430(4) 0.0000 0.0262(3) Uani 1 2 d S . .
Nb3 Nb 0.12185(6) 0.32300(3) 0.11011(2) 0.0309(2) Uani 1 1 d . . .
Nb4 Nb 0.24433(6) 0.23205(3) 0.05618(2) 0.0276(2) Uani 1 1 d . . .
Nb5 Nb 0.11364(6) 0.12393(3) 0.11052(3) 0.0327(2) Uani 1 1 d . . .
Ge1 Ge 0.0000 0.22610(5) 0.04968(4) 0.0217(3) Uani 1 2 d S . .
Ge2 Ge 0.17622(10) 0.12133(5) 0.0000 0.0309(3) Uani 1 2 d S . .
Cu1 Cu 0.2500 0.2500 0.2500 0.0454(5) Uani 1 2 d S . .
Cu2 Cu 0.0000 0.5000 0.0000 0.0579(12) Uani 1 8 d S . .
Na1 Na 0.0000 0.0669(4) 0.0000 0.051(2) Uani 1 4 d S . .
Na2 Na 0.2024(6) 0.0000 0.0535(3) 0.066(2) Uani 1 2 d S . .
Na3 Na 0.0000 0.0000 0.1676(8) 0.058(6) Uani 0.40 4 d SPU . .
Na4 Na 0.0000 0.4017(8) 0.1972(5) 0.050(5) Uani 0.32 2 d SP . .
Na5 Na 0.3905(14) 0.3200(8) 0.1350(7) 0.055(5) Uani 0.24 1 d PU . .
O1 O 0.1853(5) 0.0756(3) 0.1302(3) 0.051(2) Uani 1 1 d . . .
O2 O 0.0955(4) 0.2643(2) 0.04975(18) 0.0249(13) Uani 1 1 d . . .
O3 O 0.2368(6) 0.2807(3) 0.0000 0.0287(19) Uani 1 2 d S . .
O4 O 0.0884(5) 0.2677(3) 0.14661(19) 0.0343(15) Uani 1 1 d . . .
O5 O 0.0000 0.3343(4) 0.0000 0.027(3) Uani 1 4 d S . .
O6 O 0.1980(4) 0.1790(3) 0.0907(2) 0.0325(14) Uani 1 1 d . . .
O7 O 0.0000 0.1840(3) 0.0942(3) 0.0254(18) Uani 1 2 d S . .
O8 O 0.1593(6) 0.3698(3) 0.1483(2) 0.0473(19) Uani 1 1 d . . .
O9 O 0.0000 0.3432(4) 0.1014(3) 0.034(2) Uani 1 2 d S . .
O10 O 0.2079(6) 0.1864(3) 0.0000 0.0277(19) Uani 1 2 d S . .
O11 O 0.1142(5) 0.1033(3) 0.0452(2) 0.0353(15) Uani 1 1 d . . .
O12 O 0.3598(5) 0.2193(3) 0.0564(2) 0.0420(17) Uani 1 1 d . . .
O13 O 0.0000 0.1910(4) 0.0000 0.023(2) Uani 1 4 d S . .
O14 O 0.2397(5) 0.2881(3) 0.0960(2) 0.0353(15) Uani 1 1 d . . .
O15 O 0.0000 0.0862(4) 0.1154(3) 0.038(2) Uani 1 2 d S . .
O16 O 0.0000 0.2288(4) 0.2251(3) 0.041(2) Uani 1 2 d S . .
O17 O 0.2730(7) 0.0828(4) 0.0000 0.048(3) Uani 1 2 d S . .
O18 O 0.1510(5) 0.3630(3) 0.04913(19) 0.0339(15) Uani 1 1 d . . .
O19 O 0.0926(5) 0.1619(3) 0.1651(2) 0.0363(16) Uani 1 1 d . . .
O1W O 0.0000 0.0000 0.0563(9) 0.108(9) Uani 1 4 d SU . .
O2W O 0.3687(9) 0.3179(5) 0.2251(4) 0.088(4) Uani 0.90 1 d PU . .
O3W O 0.5000 0.2214(10) 0.1144(9) 0.111(8) Uiso 0.76 2 d SP . .
O4W O 0.1859(17) 0.0000 0.1912(7) 0.127(8) Uiso 0.94 2 d SP . .
O5W O 0.5000 0.2581(15) 0.0000 0.106(12) Uiso 0.72 4 d SP . .
O6W O 0.342(2) 0.0600(13) 0.0934(11) 0.120(11) Uiso 0.44 1 d P . .
O7W O 0.1115(15) 0.0827(9) 0.2303(7) 0.121(7) Uiso 0.68 1 d P . .
O8W O 0.5000 0.094(2) 0.1386(18) 0.125(18) Uiso 0.40 2 d SP . .
C1 C 0.0000 0.4738(12) 0.0867(8) 0.152(14) Uani 1 2 d SDU . .
C2 C 0.1463(13) 0.3357(7) 0.2755(5) 0.089(5) Uani 1 1 d U . .
H2A H 0.1806 0.3669 0.2710 0.106 Uiso 1 1 calc R . .
H2B H 0.0846 0.3457 0.2781 0.106 Uiso 1 1 calc R . .
C3 C 0.1730(11) 0.3127(7) 0.3153(4) 0.082(5) Uani 1 1 d . . .
H3A H 0.1226 0.2947 0.3279 0.098 Uiso 1 1 calc R . .
H3B H 0.1898 0.3397 0.3358 0.098 Uiso 1 1 calc R . .
N1 N 0.2441(7) 0.2775(4) 0.3118(3) 0.048(2) Uani 1 1 d . . .
H1C H 0.2363 0.2513 0.3309 0.058 Uiso 1 1 calc R . .
H1D H 0.2952 0.2935 0.3186 0.058 Uiso 1 1 calc R . .
N2 N 0.0000 0.4481(6) 0.0491(5) 0.071(5) Uani 1 2 d SD . .
N3 N 0.1564(7) 0.3028(4) 0.2373(3) 0.050(2) Uani 1 1 d . . .
H3C H 0.1721 0.3218 0.2137 0.060 Uiso 1 1 calc R . .
H3D H 0.1048 0.2870 0.2312 0.060 Uiso 1 1 calc R . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Nb1 0.0291(7) 0.0486(7) 0.0190(5) 0.0062(5) 0.000 0.000
Nb2 0.0321(7) 0.0266(5) 0.0198(5) 0.000 0.000 -0.0056(5)
Nb3 0.0343(5) 0.0376(5) 0.0208(4) -0.0042(3) -0.0019(3) -0.0063(4)
Nb4 0.0231(4) 0.0374(4) 0.0224(4) 0.0006(3) -0.0026(3) -0.0036(3)
Nb5 0.0282(5) 0.0365(5) 0.0333(4) 0.0130(3) -0.0016(3) 0.0027(4)
Ge1 0.0218(7) 0.0255(6) 0.0177(5) 0.0016(5) 0.000 0.000
Ge2 0.0287(8) 0.0302(7) 0.0337(7) 0.000 0.000 0.0017(6)
Cu1 0.0382(12) 0.0704(13) 0.0277(8) -0.0068(8) -0.0094(7) 0.0047(9)
Cu2 0.091(4) 0.0317(19) 0.051(2) 0.000 0.000 0.000
Na1 0.032(5) 0.049(5) 0.071(6) 0.000 0.000 0.000
Na2 0.083(6) 0.034(3) 0.080(5) 0.000 0.017(4) 0.000
Na3 0.080(11) 0.041(8) 0.053(9) 0.000 0.000 0.000
Na4 0.054(13) 0.070(13) 0.026(8) -0.029(9) 0.000 0.000
Na5 0.051(6) 0.062(6) 0.053(6) -0.003(4) -0.005(4) -0.008(5)
O1 0.039(5) 0.055(5) 0.060(5) 0.019(4) -0.007(4) 0.007(4)
O2 0.024(3) 0.031(3) 0.020(3) 0.001(2) -0.003(2) -0.004(3)
O3 0.026(5) 0.038(5) 0.022(4) 0.000 0.000 -0.010(4)
O4 0.033(4) 0.045(4) 0.025(3) 0.003(3) -0.003(3) -0.006(3)
O5 0.028(7) 0.022(6) 0.030(6) 0.000 0.000 0.000
O6 0.027(4) 0.042(4) 0.028(3) 0.006(3) -0.004(3) 0.000(3)
O7 0.023(5) 0.034(5) 0.019(4) 0.006(3) 0.000 0.000
O8 0.054(5) 0.054(5) 0.034(4) -0.014(3) 0.000(3) -0.013(4)
O9 0.038(6) 0.038(5) 0.028(4) -0.001(4) 0.000 0.000
O10 0.023(5) 0.035(5) 0.025(4) 0.000 0.000 -0.002(4)
O11 0.031(4) 0.039(4) 0.036(3) 0.010(3) 0.000(3) 0.000(3)
O12 0.027(4) 0.061(5) 0.038(4) 0.001(3) -0.001(3) 0.000(3)
O13 0.024(7) 0.021(5) 0.024(6) 0.000 0.000 0.000
O14 0.032(4) 0.044(4) 0.030(3) -0.005(3) 0.000(3) -0.003(3)
O15 0.038(6) 0.040(5) 0.038(5) 0.012(4) 0.000 0.000
O16 0.037(6) 0.063(7) 0.024(4) 0.009(4) 0.000 0.000
O17 0.034(6) 0.055(7) 0.055(6) 0.000 0.000 0.020(5)
O18 0.044(4) 0.036(3) 0.022(3) -0.002(3) -0.001(3) -0.007(3)
O19 0.032(4) 0.052(4) 0.025(3) 0.011(3) -0.001(3) 0.004(3)
O1W 0.111(12) 0.107(11) 0.107(11) 0.000 0.000 0.000
O2W 0.079(7) 0.100(7) 0.087(6) 0.025(6) -0.025(6) -0.009(6)
C1 0.161(17) 0.144(17) 0.151(16) 0.015(9) 0.000 0.000
C2 0.099(9) 0.098(8) 0.069(7) -0.011(7) -0.010(7) 0.023(7)
C3 0.065(10) 0.147(15) 0.033(6) -0.021(8) -0.008(6) 0.037(10)
N1 0.038(6) 0.078(7) 0.028(4) -0.005(4) -0.012(4) 0.000(5)
N2 0.133(17) 0.037(7) 0.043(8) 0.010(6) 0.000 0.000
N3 0.055(7) 0.064(6) 0.031(4) -0.001(4) -0.009(4) 0.009(5)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 O16 1.787(9) . ?
Nb1 O19 1.974(7) 12 ?
Nb1 O19 1.974(7) . ?
Nb1 O4 1.997(7) . ?
Nb1 O4 1.997(7) 12 ?
Nb1 O7 2.356(8) . ?
Nb2 O18 1.836(6) . ?
Nb2 O18 1.836(6) 10 ?
Nb2 O5 1.910(2) . ?
Nb2 O3 2.028(10) . ?
Nb2 O2 2.211(6) 10 ?
Nb2 O2 2.211(6) . ?
Nb2 Nb3 3.3347(10) 10 ?
Nb2 Nb3 3.3347(10) . ?
Nb3 O8 1.769(7) . ?
Nb3 O4 1.880(6) . ?
Nb3 O9 1.931(3) . ?
Nb3 O14 2.041(7) . ?
Nb3 O18 2.163(6) . ?
Nb3 O2 2.411(6) . ?
Nb4 O12 1.775(8) . ?
Nb4 O6 1.864(6) . ?
Nb4 O14 1.891(6) . ?
Nb4 O3 2.121(5) . ?
Nb4 O10 2.145(5) . ?
Nb4 O2 2.407(6) . ?
Nb5 O1 1.760(7) . ?
Nb5 O19 1.951(7) . ?
Nb5 O15 1.981(5) . ?
Nb5 O6 2.005(7) . ?
Nb5 O11 2.050(7) . ?
Nb5 O7 2.369(6) . ?
Ge1 O7 1.736(8) . ?
Ge1 O2 1.750(6) . ?
Ge1 O2 1.750(6) 12 ?
Ge1 O13 1.757(6) . ?
Ge2 O11 1.722(7) 10 ?
Ge2 O11 1.722(7) . ?
Ge2 O10 1.752(9) . ?
Ge2 O17 1.771(10) . ?
Ge2 Na1 3.013(5) . ?
Ge2 Na2 3.559(4) 10 ?
Ge2 Na2 3.559(4) . ?
Cu1 N3 2.004(10) 13 ?
Cu1 N3 2.004(10) . ?
Cu1 N1 2.004(8) 13 ?
Cu1 N1 2.004(8) . ?
Cu2 N2 2.007(14) 10 ?
Cu2 N2 2.007(14) 9_565 ?
Cu2 N2 2.007(14) 2_565 ?
Cu2 N2 2.007(14) . ?
Na1 O11 2.395(8) 3 ?
Na1 O11 2.395(8) . ?
Na1 O11 2.395(8) 10 ?
Na1 O11 2.395(8) 12 ?
Na1 O1W 2.43(2) 9 ?
Na1 O1W 2.43(2) . ?
Na1 Ge2 3.013(5) 3 ?
Na1 Na1 3.467(18) 9 ?
Na1 Na2 3.870(9) 9 ?
Na1 Na2 3.870(9) . ?
Na1 Na2 3.870(9) 2 ?
Na2 O6W 2.88(4) . ?
Na2 O6W 2.88(4) 11 ?
Na2 O17 2.891(11) . ?
Na2 O17 2.891(11) 11 ?
Na2 O11 3.001(8) . ?
Na2 O11 3.001(8) 11 ?
Na2 Na2 3.239(15) 10 ?
Na2 Ge2 3.559(4) 11 ?
Na2 Na1 3.870(9) 9 ?
Na3 O15 2.736(17) . ?
Na3 O15 2.736(17) 2 ?
Na3 O4W 2.90(3) . ?
Na3 O4W 2.90(3) 2 ?
Na4 O8 2.943(12) 12 ?
Na4 O8 2.943(12) . ?
Na5 O14 2.69(2) . ?
Na5 O2W 2.75(2) . ?
Na5 Na5 3.31(4) 12_655 ?
O3 Nb4 2.121(5) 10 ?
O5 Nb2 1.910(2) 3 ?
O7 Nb5 2.369(6) 12 ?
O9 Nb3 1.931(3) 12 ?
O10 Nb4 2.145(5) 10 ?
O13 Ge1 1.757(6) 10 ?
O15 Nb5 1.981(5) 12 ?
O17 Na2 2.891(11) 10 ?
O1W Na1 2.43(2) 9 ?
C1 N2 1.318(10) . ?
C1 C1 1.36(6) 2_565 ?
C2 C3 1.40(2) . ?
C2 N3 1.446(17) . ?
C3 N1 1.413(17) . ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O16 Nb1 O19 99.5(3) . 12 ?
O16 Nb1 O19 99.5(3) . . ?
O19 Nb1 O19 90.2(4) 12 . ?
O16 Nb1 O4 100.2(3) . . ?
O19 Nb1 O4 160.1(3) 12 . ?
O19 Nb1 O4 89.6(3) . . ?
O16 Nb1 O4 100.2(3) . 12 ?
O19 Nb1 O4 89.6(3) 12 12 ?
O19 Nb1 O4 160.1(3) . 12 ?
O4 Nb1 O4 83.9(4) . 12 ?
O16 Nb1 O7 170.6(4) . . ?
O19 Nb1 O7 74.1(2) 12 . ?
O19 Nb1 O7 74.1(2) . . ?
O4 Nb1 O7 86.7(2) . . ?
O4 Nb1 O7 86.7(2) 12 . ?
O18 Nb2 O18 108.2(4) . 10 ?
O18 Nb2 O5 97.8(3) . . ?
O18 Nb2 O5 97.8(3) 10 . ?
O18 Nb2 O3 97.4(3) . . ?
O18 Nb2 O3 97.4(3) 10 . ?
O5 Nb2 O3 153.9(4) . . ?
O18 Nb2 O2 168.4(3) . 10 ?
O18 Nb2 O2 82.9(3) 10 10 ?
O5 Nb2 O2 83.9(3) . 10 ?
O3 Nb2 O2 77.1(2) . 10 ?
O18 Nb2 O2 82.9(3) . . ?
O18 Nb2 O2 168.4(3) 10 . ?
O5 Nb2 O2 83.9(3) . . ?
O3 Nb2 O2 77.1(2) . . ?
O2 Nb2 O2 85.9(3) 10 . ?
O18 Nb2 Nb3 145.0(2) . 10 ?
O18 Nb2 Nb3 36.8(2) 10 10 ?
O5 Nb2 Nb3 89.20(3) . 10 ?
O3 Nb2 Nb3 90.41(3) . 10 ?
O2 Nb2 Nb3 46.25(15) 10 10 ?
O2 Nb2 Nb3 132.15(15) . 10 ?
O18 Nb2 Nb3 36.8(2) . . ?
O18 Nb2 Nb3 145.0(2) 10 . ?
O5 Nb2 Nb3 89.20(3) . . ?
O3 Nb2 Nb3 90.41(3) . . ?
O2 Nb2 Nb3 132.15(15) 10 . ?
O2 Nb2 Nb3 46.25(15) . . ?
Nb3 Nb2 Nb3 177.89(5) 10 . ?
O8 Nb3 O4 103.0(3) . . ?
O8 Nb3 O9 102.0(4) . . ?
O4 Nb3 O9 91.8(3) . . ?
O8 Nb3 O14 99.3(3) . . ?
O4 Nb3 O14 91.1(3) . . ?
O9 Nb3 O14 157.3(3) . . ?
O8 Nb3 O18 99.5(3) . . ?
O4 Nb3 O18 157.3(3) . . ?
O9 Nb3 O18 87.0(3) . . ?
O14 Nb3 O18 81.8(3) . . ?
O8 Nb3 O2 168.9(3) . . ?
O4 Nb3 O2 85.4(2) . . ?
O9 Nb3 O2 84.8(3) . . ?
O14 Nb3 O2 72.9(2) . . ?
O18 Nb3 O2 71.9(2) . . ?
O8 Nb3 Nb2 130.0(2) . . ?
O4 Nb3 Nb2 126.84(19) . . ?
O9 Nb3 Nb2 82.8(3) . . ?
O14 Nb3 Nb2 77.44(18) . . ?
O18 Nb3 Nb2 30.53(17) . . ?
O2 Nb3 Nb2 41.49(14) . . ?
O12 Nb4 O6 103.3(3) . . ?
O12 Nb4 O14 100.2(3) . . ?
O6 Nb4 O14 101.2(3) . . ?
O12 Nb4 O3 99.6(3) . . ?
O6 Nb4 O3 150.3(3) . . ?
O14 Nb4 O3 93.0(3) . . ?
O12 Nb4 O10 98.8(3) . . ?
O6 Nb4 O10 86.6(3) . . ?
O14 Nb4 O10 157.1(3) . . ?
O3 Nb4 O10 71.2(3) . . ?
O12 Nb4 O2 169.4(3) . . ?
O6 Nb4 O2 87.2(3) . . ?
O14 Nb4 O2 75.5(3) . . ?
O3 Nb4 O2 71.2(3) . . ?
O10 Nb4 O2 83.6(3) . . ?
O1 Nb5 O19 99.9(3) . . ?
O1 Nb5 O15 99.0(4) . . ?
O19 Nb5 O15 92.6(4) . . ?
O1 Nb5 O6 102.5(3) . . ?
O19 Nb5 O6 89.9(3) . . ?
O15 Nb5 O6 157.6(3) . . ?
O1 Nb5 O11 98.0(3) . . ?
O19 Nb5 O11 162.0(3) . . ?
O15 Nb5 O11 86.9(3) . . ?
O6 Nb5 O11 83.9(3) . . ?
O1 Nb5 O7 169.7(3) . . ?
O19 Nb5 O7 74.1(3) . . ?
O15 Nb5 O7 73.3(3) . . ?
O6 Nb5 O7 86.0(2) . . ?
O11 Nb5 O7 88.5(3) . . ?
O7 Ge1 O2 110.8(2) . . ?
O7 Ge1 O2 110.8(2) . 12 ?
O2 Ge1 O2 111.0(4) . 12 ?
O7 Ge1 O13 109.9(4) . . ?
O2 Ge1 O13 107.1(2) . . ?
O2 Ge1 O13 107.1(2) 12 . ?
O11 Ge2 O11 105.2(5) 10 . ?
O11 Ge2 O10 114.2(3) 10 . ?
O11 Ge2 O10 114.2(3) . . ?
O11 Ge2 O17 107.2(3) 10 . ?
O11 Ge2 O17 107.2(3) . . ?
O10 Ge2 O17 108.5(5) . . ?
O11 Ge2 Na1 52.6(2) 10 . ?
O11 Ge2 Na1 52.6(2) . . ?
O10 Ge2 Na1 133.8(3) . . ?
O17 Ge2 Na1 117.7(4) . . ?
O11 Ge2 Na2 57.3(3) 10 10 ?
O11 Ge2 Na2 100.5(3) . 10 ?
O10 Ge2 Na2 145.1(2) . 10 ?
O17 Ge2 Na2 53.8(4) . 10 ?
Na1 Ge2 Na2 71.6(2) . 10 ?
O11 Ge2 Na2 100.5(3) 10 . ?
O11 Ge2 Na2 57.3(3) . . ?
O10 Ge2 Na2 145.1(2) . . ?
O17 Ge2 Na2 53.8(4) . . ?
Na1 Ge2 Na2 71.6(2) . . ?
Na2 Ge2 Na2 54.1(2) 10 . ?
N3 Cu1 N3 180.0(5) 13 . ?
N3 Cu1 N1 84.5(4) 13 13 ?
N3 Cu1 N1 95.5(4) . 13 ?
N3 Cu1 N1 95.5(4) 13 . ?
N3 Cu1 N1 84.5(4) . . ?
N1 Cu1 N1 180.00(17) 13 . ?
N2 Cu2 N2 84.3(9) 10 9_565 ?
N2 Cu2 N2 180.0(8) 10 2_565 ?
N2 Cu2 N2 95.7(9) 9_565 2_565 ?
N2 Cu2 N2 95.7(9) 10 . ?
N2 Cu2 N2 180.0(8) 9_565 . ?
N2 Cu2 N2 84.3(9) 2_565 . ?
O11 Na1 O11 133.6(5) 3 . ?
O11 Na1 O11 92.1(4) 3 10 ?
O11 Na1 O11 69.6(3) . 10 ?
O11 Na1 O11 69.6(3) 3 12 ?
O11 Na1 O11 92.1(4) . 12 ?
O11 Na1 O11 133.6(5) 10 12 ?
O11 Na1 O1W 83.1(3) 3 9 ?
O11 Na1 O1W 132.9(2) . 9 ?
O11 Na1 O1W 83.1(3) 10 9 ?
O11 Na1 O1W 132.9(2) 12 9 ?
O11 Na1 O1W 132.9(2) 3 . ?
O11 Na1 O1W 83.1(3) . . ?
O11 Na1 O1W 132.9(2) 10 . ?
O11 Na1 O1W 83.1(3) 12 . ?
O1W Na1 O1W 89.1(9) 9 . ?
O11 Na1 Ge2 116.9(3) 3 . ?
O11 Na1 Ge2 34.83(17) . . ?
O11 Na1 Ge2 34.83(17) 10 . ?
O11 Na1 Ge2 116.9(3) 12 . ?
O1W Na1 Ge2 109.50(16) 9 . ?
O1W Na1 Ge2 109.50(16) . . ?
O11 Na1 Ge2 34.83(17) 3 3 ?
O11 Na1 Ge2 116.9(3) . 3 ?
O11 Na1 Ge2 116.9(3) 10 3 ?
O11 Na1 Ge2 34.83(17) 12 3 ?
O1W Na1 Ge2 109.50(16) 9 3 ?
O1W Na1 Ge2 109.50(16) . 3 ?
Ge2 Na1 Ge2 124.1(3) . 3 ?
O11 Na1 Na1 113.2(3) 3 9 ?
O11 Na1 Na1 113.2(3) . 9 ?
O11 Na1 Na1 113.2(3) 10 9 ?
O11 Na1 Na1 113.2(3) 12 9 ?
O1W Na1 Na1 44.5(5) 9 9 ?
O1W Na1 Na1 44.5(5) . 9 ?
Ge2 Na1 Na1 117.93(16) . 9 ?
Ge2 Na1 Na1 117.93(16) 3 9 ?
O11 Na1 Na2 50.84(19) 3 9 ?
O11 Na1 Na2 169.9(2) . 9 ?
O11 Na1 Na2 120.4(2) 10 9 ?
O11 Na1 Na2 81.2(2) 12 9 ?
O1W Na1 Na2 52.20(13) 9 9 ?
O1W Na1 Na2 88.5(3) . 9 ?
Ge2 Na1 Na2 155.21(11) . 9 ?
Ge2 Na1 Na2 60.78(9) 3 9 ?
Na1 Na1 Na2 63.38(14) 9 9 ?
O11 Na1 Na2 169.9(2) 3 . ?
O11 Na1 Na2 50.84(19) . . ?
O11 Na1 Na2 81.2(2) 10 . ?
O11 Na1 Na2 120.4(2) 12 . ?
O1W Na1 Na2 88.5(3) 9 . ?
O1W Na1 Na2 52.20(13) . . ?
Ge2 Na1 Na2 60.78(9) . . ?
Ge2 Na1 Na2 155.21(11) 3 . ?
Na1 Na1 Na2 63.38(14) 9 . ?
Na2 Na1 Na2 126.8(3) 9 . ?
O11 Na1 Na2 81.2(2) 3 2 ?
O11 Na1 Na2 120.4(2) . 2 ?
O11 Na1 Na2 169.9(2) 10 2 ?
O11 Na1 Na2 50.84(19) 12 2 ?
O1W Na1 Na2 88.5(3) 9 2 ?
O1W Na1 Na2 52.20(13) . 2 ?
Ge2 Na1 Na2 155.21(11) . 2 ?
Ge2 Na1 Na2 60.78(9) 3 2 ?
Na1 Na1 Na2 63.38(14) 9 2 ?
Na2 Na1 Na2 49.5(2) 9 2 ?
Na2 Na1 Na2 104.4(2) . 2 ?
O6W Na2 O6W 65.3(14) . 11 ?
O6W Na2 O17 64.2(7) . . ?
O6W Na2 O17 111.5(8) 11 . ?
O6W Na2 O17 111.5(8) . 11 ?
O6W Na2 O17 64.2(7) 11 11 ?
O17 Na2 O17 95.8(4) . 11 ?
O6W Na2 O11 83.0(7) . . ?
O6W Na2 O11 147.2(7) 11 . ?
O17 Na2 O11 57.0(2) . . ?
O17 Na2 O11 141.1(3) 11 . ?
O6W Na2 O11 147.2(7) . 11 ?
O6W Na2 O11 83.0(7) 11 11 ?
O17 Na2 O11 141.1(3) . 11 ?
O17 Na2 O11 57.0(2) 11 11 ?
O11 Na2 O11 126.3(4) . 11 ?
O6W Na2 Na2 114.8(7) . 10 ?
O6W Na2 Na2 114.8(7) 11 10 ?
O17 Na2 Na2 55.94(19) . 10 ?
O17 Na2 Na2 55.94(19) 11 10 ?
O11 Na2 Na2 85.19(19) . 10 ?
O11 Na2 Na2 85.19(19) 11 10 ?
O6W Na2 Ge2 138.5(7) . 11 ?
O6W Na2 Ge2 78.2(7) 11 11 ?
O17 Na2 Ge2 116.2(3) . 11 ?
O17 Na2 Ge2 29.6(2) 11 11 ?
O11 Na2 Ge2 134.5(3) . 11 ?
O11 Na2 Ge2 28.87(13) 11 11 ?
Na2 Na2 Ge2 62.94(11) 10 11 ?
O6W Na2 Ge2 78.2(7) . . ?
O6W Na2 Ge2 138.5(7) 11 . ?
O17 Na2 Ge2 29.6(2) . . ?
O17 Na2 Ge2 116.2(3) 11 . ?
O11 Na2 Ge2 28.87(13) . . ?
O11 Na2 Ge2 134.5(3) 11 . ?
Na2 Na2 Ge2 62.94(11) 10 . ?
Ge2 Na2 Ge2 124.1(2) 11 . ?
O6W Na2 Na1 173.7(7) . 9 ?
O6W Na2 Na1 120.7(7) 11 9 ?
O17 Na2 Na1 112.9(3) . 9 ?
O17 Na2 Na1 74.0(3) 11 9 ?
O11 Na2 Na1 90.8(3) . 9 ?
O11 Na2 Na1 38.2(2) 11 9 ?
Na2 Na2 Na1 65.26(11) 10 9 ?
Ge2 Na2 Na1 47.62(14) 11 9 ?
Ge2 Na2 Na1 96.8(2) . 9 ?
O6W Na2 Na1 120.7(7) . . ?
O6W Na2 Na1 173.7(7) 11 . ?
O17 Na2 Na1 74.0(3) . . ?
O17 Na2 Na1 112.9(3) 11 . ?
O11 Na2 Na1 38.2(2) . . ?
O11 Na2 Na1 90.8(3) 11 . ?
Na2 Na2 Na1 65.26(11) 10 . ?
Ge2 Na2 Na1 96.8(2) 11 . ?
Ge2 Na2 Na1 47.62(14) . . ?
Na1 Na2 Na1 53.2(3) 9 . ?
O15 Na3 O15 109.4(9) . 2 ?
O15 Na3 O4W 98.2(3) . . ?
O15 Na3 O4W 98.2(3) 2 . ?
O15 Na3 O4W 98.2(3) . 2 ?
O15 Na3 O4W 98.2(3) 2 2 ?
O4W Na3 O4W 151.5(13) . 2 ?
O8 Na4 O8 109.7(6) 12 . ?
O14 Na5 O2W 109.1(8) . . ?
O14 Na5 Na5 147.7(5) . 12_655 ?
O2W Na5 Na5 96.9(5) . 12_655 ?
Ge1 O2 Nb2 124.4(3) . . ?
Ge1 O2 Nb4 125.0(3) . . ?
Nb2 O2 Nb4 96.3(2) . . ?
Ge1 O2 Nb3 119.6(3) . . ?
Nb2 O2 Nb3 92.3(2) . . ?
Nb4 O2 Nb3 90.2(2) . . ?
Nb2 O3 Nb4 112.1(3) . 10 ?
Nb2 O3 Nb4 112.1(3) . . ?
Nb4 O3 Nb4 106.7(4) 10 . ?
Nb3 O4 Nb1 151.4(4) . . ?
Nb2 O5 Nb2 164.4(7) . 3 ?
Nb4 O6 Nb5 158.7(4) . . ?
Ge1 O7 Nb1 120.7(4) . . ?
Ge1 O7 Nb5 125.1(2) . . ?
Nb1 O7 Nb5 91.9(2) . . ?
Ge1 O7 Nb5 125.1(2) . 12 ?
Nb1 O7 Nb5 91.9(2) . 12 ?
Nb5 O7 Nb5 92.9(3) . 12 ?
Nb3 O8 Na4 105.1(4) . . ?
Nb3 O9 Nb3 144.7(5) 12 . ?
Ge2 O10 Nb4 126.96(19) . . ?
Ge2 O10 Nb4 126.96(19) . 10 ?
Nb4 O10 Nb4 105.0(4) . 10 ?
Ge2 O11 Nb5 134.3(4) . . ?
Ge2 O11 Na1 92.6(3) . . ?
Nb5 O11 Na1 130.6(3) . . ?
Ge2 O11 Na2 93.9(3) . . ?
Nb5 O11 Na2 98.8(3) . . ?
Na1 O11 Na2 90.9(3) . . ?
Ge1 O13 Ge1 117.7(6) 10 . ?
Nb4 O14 Nb3 120.4(3) . . ?
Nb4 O14 Na5 118.9(6) . . ?
Nb3 O14 Na5 120.6(5) . . ?
Nb5 O15 Nb5 120.1(5) . 12 ?
Nb5 O15 Na3 116.5(3) . . ?
Nb5 O15 Na3 116.5(3) 12 . ?
Ge2 O17 Na2 96.6(4) . 10 ?
Ge2 O17 Na2 96.6(4) . . ?
Na2 O17 Na2 68.1(4) 10 . ?
Nb2 O18 Nb3 112.7(3) . . ?
Nb5 O19 Nb1 119.8(3) . . ?
Na1 O1W Na1 90.9(9) 9 . ?
N2 C1 C1 120.4(16) . 2_565 ?
C3 C2 N3 113.9(14) . . ?
C2 C3 N1 115.3(12) . . ?
C3 N1 Cu1 109.5(7) . . ?
C1 N2 Cu2 107.5(18) . . ?
C2 N3 Cu1 108.9(8) . . ?
_diffrn_measured_fraction_theta_max 0.990
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.990
_refine_diff_density_max         3.341
_refine_diff_density_min         -1.481
_refine_diff_density_rms         0.238


data_2
_database_code_depnum_ccdc_archive 'CCDC 912235'
#TrackingRef 'Compound-2.CIF'
_audit_creation_method           SHELXL-97
_chemical_name_systematic        
;
?
;
_chemical_name_common            ?
_chemical_melting_point          ?
_chemical_formula_moiety         ?
_chemical_formula_sum            'C10 H58 Cu2.50 N10 Na3 Nb6 O28'
_chemical_formula_weight         1551.94
loop_
_atom_type_symbol
_atom_type_description
_atom_type_scat_dispersion_real
_atom_type_scat_dispersion_imag
_atom_type_scat_source
C C 0.0033 0.0016 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
H H 0.0000 0.0000 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
N N 0.0061 0.0033 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
O O 0.0106 0.0060 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Nb Nb -2.0727 0.6215 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Cu Cu 0.3201 1.2651 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
Na Na 0.0362 0.0249 'International Tables Vol C Tables 4.2.6.8 and 6.1.1.4'
_symmetry_cell_setting           Monoclinic
_symmetry_space_group_name_H-M   P2(1)/n
loop_
_symmetry_equiv_pos_as_xyz
'x, y, z'
'-x+1/2, y+1/2, -z+1/2'
'-x, -y, -z'
'x-1/2, -y-1/2, z-1/2'
_cell_length_a                   13.092(3)
_cell_length_b                   20.171(4)
_cell_length_c                   17.283(4)
_cell_angle_alpha                90.00
_cell_angle_beta                 100.25(3)
_cell_angle_gamma                90.00
_cell_volume                     4491.2(16)
_cell_formula_units_Z            4
_cell_measurement_temperature    293(2)
_cell_measurement_reflns_used    10240
_cell_measurement_theta_min      3.13
_cell_measurement_theta_max      27.48
_exptl_crystal_description       block
_exptl_crystal_colour            purple
_exptl_crystal_size_max          0.25
_exptl_crystal_size_mid          0.13
_exptl_crystal_size_min          0.12
_exptl_crystal_density_meas      ?
_exptl_crystal_density_diffrn    2.295
_exptl_crystal_density_method    'not measured'
_exptl_crystal_F_000             3054
_exptl_absorpt_coefficient_mu    2.755
_exptl_absorpt_correction_type   multi-scan
_exptl_absorpt_correction_T_min  0.552
_exptl_absorpt_correction_T_max  0.745
_exptl_absorpt_process_details   'ABSCOR by T.Higashi 8 March, 1995'
_exptl_special_details           
;
?
;
_diffrn_ambient_temperature      293(2)
_diffrn_radiation_wavelength     0.71073
_diffrn_radiation_type           MoK\a
_diffrn_radiation_source         'fine-focus sealed tube'
_diffrn_radiation_monochromator  graphite
_diffrn_measurement_device_type  'Rigaku R-AXIS RAPID IP'
_diffrn_measurement_method       Oscillation
_diffrn_detector_area_resol_mean 0.01
_diffrn_standards_number         0
_diffrn_standards_interval_count 0
_diffrn_standards_interval_time  0
_diffrn_standards_decay_%        none
_diffrn_reflns_number            42369
_diffrn_reflns_av_R_equivalents  0.0578
_diffrn_reflns_av_unetI/netI     0.0491
_diffrn_reflns_limit_h_min       -16
_diffrn_reflns_limit_h_max       16
_diffrn_reflns_limit_k_min       -26
_diffrn_reflns_limit_k_max       26
_diffrn_reflns_limit_l_min       -22
_diffrn_reflns_limit_l_max       22
_diffrn_reflns_theta_min         3.13
_diffrn_reflns_theta_max         27.48
_reflns_number_total             10240
_reflns_number_gt                8125
_reflns_threshold_expression     >2sigma(I)
_computing_data_collection       auto
_computing_cell_refinement       auto
_computing_data_reduction        auto
_computing_structure_solution    'SHELXS-97 (Sheldrick, 1990)'
_computing_structure_refinement  'SHELXL-97 (Sheldrick, 1997)'
_computing_molecular_graphics    ?
_computing_publication_material  ?
_refine_special_details          
;
Refinement of F^2^ against ALL reflections. The weighted R-factor wR and
goodness of fit S are based on F^2^, conventional R-factors R are based
on F, with F set to zero for negative F^2^. The threshold expression of
F^2^ > 2sigma(F^2^) is used only for calculating R-factors(gt) etc. and is
not relevant to the choice of reflections for refinement. R-factors based
on F^2^ are statistically about twice as large as those based on F, and R-
factors based on ALL data will be even larger.
;
_refine_ls_structure_factor_coef Fsqd
_refine_ls_matrix_type           full
_refine_ls_weighting_scheme      calc
_refine_ls_weighting_details     
'calc w=1/[\s^2^(Fo^2^)+(0.0099P)^2^+25.1236P] where P=(Fo^2^+2Fc^2^)/3'
_atom_sites_solution_primary     direct
_atom_sites_solution_secondary   difmap
_atom_sites_solution_hydrogens   geom
_refine_ls_hydrogen_treatment    constr
_refine_ls_extinction_method     none
_refine_ls_extinction_coef       ?
_refine_ls_number_reflns         10240
_refine_ls_number_parameters     538
_refine_ls_number_restraints     0
_refine_ls_R_factor_all          0.0591
_refine_ls_R_factor_gt           0.0425
_refine_ls_wR_factor_ref         0.0813
_refine_ls_wR_factor_gt          0.0767
_refine_ls_goodness_of_fit_ref   1.128
_refine_ls_restrained_S_all      1.128
_refine_ls_shift/su_max          0.002
_refine_ls_shift/su_mean         0.000
loop_
_atom_site_label
_atom_site_type_symbol
_atom_site_fract_x
_atom_site_fract_y
_atom_site_fract_z
_atom_site_U_iso_or_equiv
_atom_site_adp_type
_atom_site_occupancy
_atom_site_symmetry_multiplicity
_atom_site_calc_flag
_atom_site_refinement_flags
_atom_site_disorder_assembly
_atom_site_disorder_group
Nb1 Nb 0.15808(3) 0.04936(2) 0.79571(3) 0.01192(10) Uani 1 1 d . . .
Nb2 Nb 0.11883(3) 0.13083(2) 0.62431(3) 0.01000(9) Uani 1 1 d . . .
Nb3 Nb 0.06726(3) -0.03982(2) 0.63725(3) 0.01006(9) Uani 1 1 d . . .
Nb4 Nb 0.35954(3) 0.10098(2) 0.71542(3) 0.01056(9) Uani 1 1 d . . .
Nb5 Nb 0.31147(3) -0.06117(2) 0.72563(3) 0.01026(9) Uani 1 1 d . . .
Nb6 Nb 0.25841(3) 0.00495(2) 0.54783(3) 0.01049(9) Uani 1 1 d . . .
Na1 Na 0.5405(3) -0.2109(2) 0.8281(2) 0.0679(10) Uani 1 1 d . . .
Na2 Na 0.6349(3) 0.1967(2) 0.8468(3) 0.0780(12) Uani 1 1 d . . .
Na3 Na 0.1036(3) 0.1238(3) 1.0212(3) 0.0858(14) Uani 1 1 d . . .
O1 O 0.1256(3) -0.03940(17) 0.5370(2) 0.0121(7) Uani 1 1 d . . .
O2 O 0.2899(3) 0.10439(18) 0.8042(2) 0.0128(7) Uani 1 1 d . . .
O3 O 0.0082(3) 0.05499(18) 0.5951(2) 0.0117(7) Uani 1 1 d . . .
O4 O 0.0464(3) -0.00597(18) 0.7386(2) 0.0141(7) Uani 1 1 d . . .
O5 O 0.4135(2) 0.01146(17) 0.7436(2) 0.0112(7) Uani 1 1 d . . .
O6 O 0.2573(3) 0.16440(18) 0.6574(2) 0.0120(7) Uani 1 1 d . . .
O7 O 0.3326(3) -0.06278(18) 0.6121(2) 0.0137(7) Uani 1 1 d . . .
O8 O 0.1756(3) 0.09584(18) 0.5246(2) 0.0135(7) Uani 1 1 d . . .
O9 O 0.1710(3) -0.10161(17) 0.6842(2) 0.0127(7) Uani 1 1 d . . .
O10 O 0.0478(3) 0.20050(18) 0.5815(2) 0.0145(7) Uani 1 1 d . . .
O11 O 0.2109(3) 0.03269(17) 0.6667(2) 0.0108(7) Uani 1 1 d . . .
O12 O 0.4713(3) 0.15089(19) 0.7418(2) 0.0177(8) Uani 1 1 d . . .
O13 O 0.2925(3) -0.00585(19) 0.4553(2) 0.0168(8) Uani 1 1 d . . .
O14 O 0.3780(3) 0.07155(18) 0.5982(2) 0.0144(7) Uani 1 1 d . . .
O15 O 0.2494(3) -0.02833(18) 0.8132(2) 0.0136(7) Uani 1 1 d . . .
O16 O 0.3840(3) -0.13013(18) 0.7682(2) 0.0162(8) Uani 1 1 d . . .
O17 O 0.0910(3) 0.12687(18) 0.7293(2) 0.0127(7) Uani 1 1 d . . .
O18 O -0.0459(3) -0.08953(18) 0.6102(2) 0.0144(7) Uani 1 1 d . . .
O19 O 0.1165(3) 0.0629(2) 0.8859(2) 0.0221(9) Uani 1 1 d . . .
O1W O 0.4231(3) 0.1145(2) 0.9461(2) 0.0263(10) Uani 1 1 d . . .
O2W O 0.5256(3) -0.2920(2) 0.6949(2) 0.0244(9) Uani 1 1 d . . .
O3W O 0.5030(3) -0.2557(2) 0.5355(3) 0.0307(10) Uani 1 1 d . . .
O4W O 0.6836(3) -0.1374(2) 0.9293(3) 0.0308(10) Uani 1 1 d . . .
O5W O 0.4730(3) -0.1168(2) 0.5218(3) 0.0300(10) Uani 1 1 d . . .
O6W O 0.1749(3) -0.1276(3) 0.1446(3) 0.0352(11) Uani 1 1 d . . .
O7W O 0.6486(3) 0.2016(2) 1.0093(3) 0.0295(10) Uani 1 1 d . . .
O8W O 0.3141(4) 0.2136(3) 0.5014(3) 0.0444(13) Uani 1 1 d . . .
O9W O -0.0897(4) -0.0079(3) 0.8761(3) 0.0489(14) Uani 1 1 d . . .
C1 C 0.1730(4) -0.2194(3) 0.5589(3) 0.0204(12) Uani 1 1 d . . .
H1A H 0.1895 -0.1725 0.5585 0.024 Uiso 1 1 calc R . .
H1B H 0.1584 -0.2350 0.5050 0.024 Uiso 1 1 calc R . .
C2 C 0.7028(4) 0.0348(3) 0.9765(3) 0.0258(13) Uani 1 1 d . . .
H2A H 0.7371 -0.0071 0.9911 0.031 Uiso 1 1 calc R . .
H2B H 0.7555 0.0689 0.9781 0.031 Uiso 1 1 calc R . .
C3 C 0.1021(5) -0.1605(3) 0.8593(4) 0.0252(13) Uani 1 1 d . . .
H3A H 0.1029 -0.1140 0.8454 0.030 Uiso 1 1 calc R . .
H3B H 0.1146 -0.1641 0.9162 0.030 Uiso 1 1 calc R . .
C4 C 0.1940(4) -0.1434(3) 0.3683(3) 0.0211(12) Uani 1 1 d . . .
H4A H 0.1414 -0.1777 0.3579 0.025 Uiso 1 1 calc R . .
H4B H 0.2015 -0.1304 0.4230 0.025 Uiso 1 1 calc R . .
C5 C 0.2965(5) -0.1689(3) 0.3508(4) 0.0251(13) Uani 1 1 d . . .
H5A H 0.3250 -0.2022 0.3890 0.030 Uiso 1 1 calc R . .
H5B H 0.2864 -0.1888 0.2988 0.030 Uiso 1 1 calc R . .
C6 C 0.2635(4) -0.2576(3) 0.6055(3) 0.0196(11) Uani 1 1 d . . .
H6A H 0.2550 -0.3046 0.5942 0.024 Uiso 1 1 calc R . .
H6B H 0.3279 -0.2432 0.5905 0.024 Uiso 1 1 calc R . .
C7 C 0.6389(5) 0.0303(3) 0.8954(3) 0.0249(13) Uani 1 1 d . . .
H7A H 0.6127 0.0738 0.8779 0.030 Uiso 1 1 calc R . .
H7B H 0.6812 0.0139 0.8587 0.030 Uiso 1 1 calc R . .
C8 C -0.0010(5) -0.1909(3) 0.8251(4) 0.0258(13) Uani 1 1 d . . .
H8A H -0.0054 -0.2355 0.8451 0.031 Uiso 1 1 calc R . .
H8B H -0.0570 -0.1648 0.8395 0.031 Uiso 1 1 calc R . .
C9 C 0.2746(5) 0.1136(3) 0.3041(4) 0.0339(15) Uani 1 1 d . . .
H9A H 0.2783 0.1285 0.3579 0.041 Uiso 1 1 calc R . .
H9B H 0.2472 0.1496 0.2693 0.041 Uiso 1 1 calc R . .
C10 C 0.3812(5) 0.0948(3) 0.2902(4) 0.0281(14) Uani 1 1 d . . .
H10A H 0.3803 0.0892 0.2343 0.034 Uiso 1 1 calc R . .
H10B H 0.4304 0.1295 0.3094 0.034 Uiso 1 1 calc R . .
N1 N 0.4125(3) 0.0322(2) 0.3319(3) 0.0198(10) Uani 1 1 d . . .
H1C H 0.4416 0.0409 0.3821 0.024 Uiso 1 1 calc R . .
H1D H 0.4599 0.0113 0.3088 0.024 Uiso 1 1 calc R . .
N2 N 0.1639(3) -0.0857(2) 0.3166(3) 0.0216(10) Uani 1 1 d . . .
H2C H 0.1097 -0.0644 0.3308 0.026 Uiso 1 1 calc R . .
H2D H 0.1460 -0.0987 0.2662 0.026 Uiso 1 1 calc R . .
N3 N 0.6319(3) 0.0515(2) 1.0318(2) 0.0174(10) Uani 1 1 d . . .
H3C H 0.6184 0.0953 1.0301 0.021 Uiso 1 1 calc R . .
H3D H 0.6617 0.0409 1.0813 0.021 Uiso 1 1 calc R . .
N4 N 0.3688(3) -0.1112(2) 0.3547(3) 0.0194(10) Uani 1 1 d . . .
H4C H 0.4120 -0.1170 0.3202 0.023 Uiso 1 1 calc R . .
H4D H 0.4073 -0.1085 0.4032 0.023 Uiso 1 1 calc R . .
N5 N 0.1832(4) -0.1967(2) 0.8269(3) 0.0191(10) Uani 1 1 d . . .
H5C H 0.1968 -0.2357 0.8520 0.023 Uiso 1 1 calc R . .
H5D H 0.2421 -0.1728 0.8336 0.023 Uiso 1 1 calc R . .
N6 N 0.2054(4) 0.0549(3) 0.2889(3) 0.0248(11) Uani 1 1 d . . .
H6C H 0.1815 0.0508 0.2370 0.030 Uiso 1 1 calc R . .
H6D H 0.1508 0.0595 0.3135 0.030 Uiso 1 1 calc R . .
N7 N -0.0093(4) -0.1922(2) 0.7385(3) 0.0199(10) Uani 1 1 d . . .
H7C H -0.0318 -0.1527 0.7181 0.024 Uiso 1 1 calc R . .
H7D H -0.0552 -0.2234 0.7176 0.024 Uiso 1 1 calc R . .
N8 N 0.2676(3) -0.2461(2) 0.6904(3) 0.0156(9) Uani 1 1 d . . .
H8C H 0.3178 -0.2164 0.7077 0.019 Uiso 1 1 calc R . .
H8D H 0.2838 -0.2842 0.7168 0.019 Uiso 1 1 calc R . .
N9 N 0.0814(3) -0.2302(2) 0.5974(3) 0.0189(10) Uani 1 1 d . . .
H9C H 0.0583 -0.2722 0.5900 0.023 Uiso 1 1 calc R . .
H9D H 0.0296 -0.2023 0.5778 0.023 Uiso 1 1 calc R . .
N10 N 0.5514(3) -0.0156(2) 0.8983(2) 0.0179(10) Uani 1 1 d . . .
H10C H 0.5727 -0.0579 0.8959 0.022 Uiso 1 1 calc R . .
H10D H 0.5000 -0.0082 0.8572 0.022 Uiso 1 1 calc R . .
Cu1 Cu 0.5000 0.0000 1.0000 0.0178(2) Uani 1 2 d S . .
Cu2 Cu 0.28809(5) -0.02622(3) 0.32953(4) 0.01525(13) Uani 1 1 d . . .
Cu3 Cu 0.13128(5) -0.21239(3) 0.71207(4) 0.01424(14) Uani 1 1 d . . .
loop_
_atom_site_aniso_label
_atom_site_aniso_U_11
_atom_site_aniso_U_22
_atom_site_aniso_U_33
_atom_site_aniso_U_23
_atom_site_aniso_U_13
_atom_site_aniso_U_12
Nb1 0.0137(2) 0.0122(2) 0.0102(2) 0.00042(17) 0.00313(17) 0.00117(18)
Nb2 0.01029(19) 0.0081(2) 0.0114(2) 0.00016(17) 0.00144(17) 0.00063(17)
Nb3 0.00884(19) 0.0090(2) 0.0119(2) 0.00144(16) 0.00067(17) -0.00042(17)
Nb4 0.00953(19) 0.0093(2) 0.0124(2) -0.00142(17) 0.00086(17) -0.00086(17)
Nb5 0.00984(19) 0.0086(2) 0.0116(2) 0.00059(17) -0.00029(17) 0.00074(17)
Nb6 0.01105(19) 0.0107(2) 0.01000(19) -0.00070(17) 0.00262(16) -0.00008(17)
Na1 0.062(2) 0.062(2) 0.080(3) 0.004(2) 0.012(2) 0.0027(19)
Na2 0.075(3) 0.079(3) 0.077(3) -0.002(2) 0.004(2) -0.007(2)
Na3 0.083(3) 0.108(4) 0.068(3) -0.009(3) 0.016(2) 0.007(3)
O1 0.0119(16) 0.0092(17) 0.0136(17) -0.0023(14) -0.0017(14) -0.0021(14)
O2 0.0136(16) 0.0131(18) 0.0109(16) -0.0030(14) 0.0007(14) -0.0009(15)
O3 0.0091(15) 0.0115(18) 0.0138(17) 0.0025(14) -0.0001(14) 0.0018(14)
O4 0.0123(16) 0.0146(19) 0.0152(17) 0.0025(15) 0.0026(14) -0.0022(15)
O5 0.0083(15) 0.0112(18) 0.0138(17) 0.0010(14) 0.0009(13) 0.0019(14)
O6 0.0108(16) 0.0114(18) 0.0129(17) -0.0015(14) -0.0004(14) -0.0002(14)
O7 0.0136(16) 0.0117(18) 0.0160(17) 0.0000(14) 0.0027(14) 0.0016(15)
O8 0.0161(17) 0.0139(18) 0.0105(16) 0.0014(14) 0.0024(14) 0.0023(15)
O9 0.0112(16) 0.0097(17) 0.0162(17) 0.0003(14) -0.0003(14) 0.0004(14)
O10 0.0169(17) 0.0118(18) 0.0141(17) 0.0018(14) 0.0012(14) 0.0046(15)
O11 0.0099(15) 0.0097(17) 0.0121(16) 0.0008(13) 0.0005(13) -0.0015(14)
O12 0.0148(17) 0.0153(19) 0.0214(19) -0.0034(15) -0.0012(15) -0.0060(15)
O13 0.0182(18) 0.018(2) 0.0138(17) -0.0009(15) 0.0028(15) -0.0007(16)
O14 0.0131(16) 0.0148(19) 0.0150(18) -0.0019(14) 0.0019(14) -0.0021(15)
O15 0.0167(17) 0.0124(18) 0.0111(16) 0.0017(14) 0.0009(14) 0.0018(15)
O16 0.0154(17) 0.0103(18) 0.0215(19) 0.0015(15) -0.0007(15) 0.0024(15)
O17 0.0121(16) 0.0147(18) 0.0114(16) 0.0003(14) 0.0024(14) 0.0013(14)
O18 0.0109(16) 0.0150(19) 0.0168(18) 0.0004(15) 0.0010(14) -0.0017(15)
O19 0.028(2) 0.027(2) 0.0136(18) 0.0009(16) 0.0092(17) 0.0064(18)
O1W 0.025(2) 0.031(2) 0.020(2) -0.0006(18) -0.0040(17) 0.0072(19)
O2W 0.025(2) 0.025(2) 0.026(2) 0.0027(18) 0.0116(18) -0.0016(18)
O3W 0.028(2) 0.034(3) 0.034(2) 0.007(2) 0.015(2) 0.006(2)
O4W 0.031(2) 0.028(2) 0.033(2) -0.003(2) 0.004(2) 0.005(2)
O5W 0.028(2) 0.031(3) 0.031(2) -0.0034(19) 0.0027(19) 0.009(2)
O6W 0.027(2) 0.046(3) 0.034(3) 0.001(2) 0.009(2) -0.004(2)
O7W 0.028(2) 0.028(2) 0.031(2) -0.0044(19) 0.0029(19) -0.0010(19)
O8W 0.043(3) 0.038(3) 0.060(3) 0.012(3) 0.030(3) 0.006(2)
O9W 0.029(2) 0.064(4) 0.055(3) 0.017(3) 0.009(2) -0.009(3)
C1 0.027(3) 0.020(3) 0.015(3) 0.001(2) 0.007(2) 0.001(2)
C2 0.021(3) 0.035(4) 0.021(3) 0.002(3) 0.002(2) -0.004(3)
C3 0.038(3) 0.018(3) 0.024(3) -0.007(2) 0.017(3) 0.004(3)
C4 0.024(3) 0.015(3) 0.028(3) 0.000(2) 0.011(2) -0.005(2)
C5 0.026(3) 0.020(3) 0.031(3) -0.003(3) 0.011(3) -0.003(3)
C6 0.022(3) 0.018(3) 0.021(3) -0.003(2) 0.008(2) 0.000(2)
C7 0.028(3) 0.030(3) 0.016(3) -0.001(2) 0.004(2) -0.002(3)
C8 0.030(3) 0.026(3) 0.026(3) -0.001(3) 0.016(3) -0.001(3)
C9 0.042(4) 0.021(3) 0.042(4) 0.009(3) 0.016(3) 0.008(3)
C10 0.026(3) 0.027(3) 0.032(3) 0.002(3) 0.009(3) -0.002(3)
N1 0.021(2) 0.018(2) 0.023(2) -0.0037(19) 0.008(2) -0.003(2)
N2 0.017(2) 0.022(3) 0.025(3) -0.011(2) 0.003(2) 0.000(2)
N3 0.021(2) 0.021(2) 0.0078(19) 0.0022(18) -0.0023(18) 0.000(2)
N4 0.017(2) 0.021(2) 0.022(2) 0.001(2) 0.0080(19) 0.003(2)
N5 0.026(2) 0.013(2) 0.017(2) 0.0017(18) 0.0005(19) 0.001(2)
N6 0.021(2) 0.028(3) 0.028(3) 0.008(2) 0.011(2) 0.006(2)
N7 0.021(2) 0.018(2) 0.022(2) 0.0021(19) 0.010(2) 0.002(2)
N8 0.016(2) 0.012(2) 0.018(2) 0.0019(18) 0.0010(18) -0.0003(18)
N9 0.019(2) 0.018(2) 0.018(2) 0.0011(19) -0.0026(19) 0.0019(19)
N10 0.019(2) 0.022(3) 0.012(2) -0.0015(18) -0.0006(18) 0.003(2)
Cu1 0.0162(4) 0.0235(5) 0.0128(4) -0.0026(4) 0.0001(4) -0.0005(4)
Cu2 0.0141(3) 0.0173(3) 0.0157(3) -0.0004(3) 0.0061(2) 0.0005(3)
Cu3 0.0148(3) 0.0143(3) 0.0139(3) 0.0005(2) 0.0031(2) 0.0019(3)
_geom_special_details            
;
All esds (except the esd in the dihedral angle between two l.s. planes)
are estimated using the full covariance matrix. The cell esds are taken
into account individually in the estimation of esds in distances, angles
and torsion angles; correlations between esds in cell parameters are only
used when they are defined by crystal symmetry. An approximate (isotropic)
treatment of cell esds is used for estimating esds involving l.s. planes.
;
loop_
_geom_bond_atom_site_label_1
_geom_bond_atom_site_label_2
_geom_bond_distance
_geom_bond_site_symmetry_2
_geom_bond_publ_flag
Nb1 O19 1.762(4) . ?
Nb1 O4 1.961(3) . ?
Nb1 O15 1.961(4) . ?
Nb1 O2 2.036(3) . ?
Nb1 O17 2.043(4) . ?
Nb1 O11 2.472(4) . ?
Nb1 Nb3 3.3153(9) . ?
Nb1 Nb2 3.3463(9) . ?
Nb1 Nb4 3.3567(10) . ?
Nb2 O10 1.773(4) . ?
Nb2 O17 1.915(3) . ?
Nb2 O6 1.924(3) . ?
Nb2 O3 2.105(3) . ?
Nb2 O8 2.116(4) . ?
Nb2 O11 2.365(3) . ?
Nb2 Nb4 3.3178(11) . ?
Nb3 O18 1.781(3) . ?
Nb3 O9 1.914(3) . ?
Nb3 O4 1.945(4) . ?
Nb3 O1 2.015(4) . ?
Nb3 O3 2.141(3) . ?
Nb3 O11 2.366(3) . ?
Nb3 Nb6 3.2928(10) . ?
Nb3 Nb5 3.3171(11) . ?
Nb4 O12 1.768(4) . ?
Nb4 O2 1.919(4) . ?
Nb4 O5 1.968(3) . ?
Nb4 O6 1.989(3) . ?
Nb4 O14 2.166(4) . ?
Nb4 O11 2.410(3) . ?
Nb4 Nb5 3.3413(9) . ?
Nb5 O16 1.769(4) . ?
Nb5 O15 1.957(4) . ?
Nb5 O5 1.970(3) . ?
Nb5 O9 2.023(3) . ?
Nb5 O7 2.030(4) . ?
Nb5 O11 2.424(3) . ?
Nb5 Nb6 3.3083(9) . ?
Nb6 O13 1.748(4) . ?
Nb6 O7 1.914(4) . ?
Nb6 O1 1.934(3) . ?
Nb6 O14 2.128(3) . ?
Nb6 O8 2.131(4) . ?
Nb6 O11 2.318(4) . ?
Na1 O16 2.678(5) . ?
Na1 O4W 2.757(6) . ?
Na1 O10 2.759(5) 2_546 ?
Na1 O2W 2.803(6) . ?
Na2 O12 2.711(5) . ?
Na2 O7W 2.785(6) . ?
Na2 O6W 2.834(6) 3_656 ?
Na2 N7 3.006(7) 2_556 ?
Na3 O19 2.673(6) . ?
Na3 O4W 2.778(6) 3_657 ?
Na3 O3W 2.886(7) 2_556 ?
Na3 O9W 2.962(7) 3_557 ?
O9 Cu3 2.363(4) . ?
O10 Na1 2.759(5) 2_556 ?
O13 Cu2 2.203(4) . ?
O3W Na3 2.886(7) 2_546 ?
O4W Na3 2.778(6) 3_657 ?
O6W Na2 2.834(6) 3_656 ?
O9W Na3 2.962(7) 3_557 ?
C1 N9 1.487(7) . ?
C1 C6 1.520(8) . ?
C2 N3 1.484(7) . ?
C2 C7 1.503(7) . ?
C3 N5 1.479(7) . ?
C3 C8 1.504(8) . ?
C4 N2 1.478(7) . ?
C4 C5 1.517(8) . ?
C5 N4 1.495(7) . ?
C6 N8 1.476(7) . ?
C7 N10 1.482(7) . ?
C8 N7 1.483(7) . ?
C9 N6 1.486(8) . ?
C9 C10 1.506(9) . ?
C10 N1 1.476(8) . ?
N1 Cu2 2.004(5) . ?
N2 Cu2 2.000(5) . ?
N3 Cu1 2.007(4) . ?
N4 Cu2 2.019(5) . ?
N5 Cu3 2.006(4) . ?
N6 Cu2 2.017(5) . ?
N7 Cu3 2.015(5) . ?
N7 Na2 3.006(7) 2_546 ?
N8 Cu3 2.007(4) . ?
N9 Cu3 2.005(4) . ?
N10 Cu1 2.015(4) . ?
Cu1 N3 2.007(4) 3_657 ?
Cu1 N10 2.015(4) 3_657 ?
loop_
_geom_angle_atom_site_label_1
_geom_angle_atom_site_label_2
_geom_angle_atom_site_label_3
_geom_angle
_geom_angle_site_symmetry_1
_geom_angle_site_symmetry_3
_geom_angle_publ_flag
O19 Nb1 O4 102.32(17) . . ?
O19 Nb1 O15 105.22(17) . . ?
O4 Nb1 O15 90.13(15) . . ?
O19 Nb1 O2 104.09(17) . . ?
O4 Nb1 O2 153.34(14) . . ?
O15 Nb1 O2 86.50(15) . . ?
O19 Nb1 O17 102.08(16) . . ?
O4 Nb1 O17 86.88(14) . . ?
O15 Nb1 O17 152.54(14) . . ?
O2 Nb1 O17 84.11(14) . . ?
O19 Nb1 O11 177.95(15) . . ?
O4 Nb1 O11 76.84(13) . . ?
O15 Nb1 O11 76.69(13) . . ?
O2 Nb1 O11 76.65(13) . . ?
O17 Nb1 O11 76.05(13) . . ?
O19 Nb1 Nb3 133.90(14) . . ?
O4 Nb1 Nb3 31.76(11) . . ?
O15 Nb1 Nb3 79.22(10) . . ?
O2 Nb1 Nb3 122.02(10) . . ?
O17 Nb1 Nb3 84.04(10) . . ?
O11 Nb1 Nb3 45.42(8) . . ?
O19 Nb1 Nb2 133.21(13) . . ?
O4 Nb1 Nb2 81.43(11) . . ?
O15 Nb1 Nb2 121.49(11) . . ?
O2 Nb1 Nb2 77.91(10) . . ?
O17 Nb1 Nb2 31.13(10) . . ?
O11 Nb1 Nb2 44.93(8) . . ?
Nb3 Nb1 Nb2 63.85(2) . . ?
O19 Nb1 Nb4 134.98(14) . . ?
O4 Nb1 Nb4 122.63(11) . . ?
O15 Nb1 Nb4 79.03(11) . . ?
O2 Nb1 Nb4 30.89(10) . . ?
O17 Nb1 Nb4 79.70(10) . . ?
O11 Nb1 Nb4 45.80(8) . . ?
Nb3 Nb1 Nb4 91.12(2) . . ?
Nb2 Nb1 Nb4 59.34(2) . . ?
O10 Nb2 O17 104.76(16) . . ?
O10 Nb2 O6 103.99(16) . . ?
O17 Nb2 O6 93.50(15) . . ?
O10 Nb2 O3 100.86(15) . . ?
O17 Nb2 O3 87.62(14) . . ?
O6 Nb2 O3 153.94(14) . . ?
O10 Nb2 O8 99.12(15) . . ?
O17 Nb2 O8 155.72(14) . . ?
O6 Nb2 O8 84.86(14) . . ?
O3 Nb2 O8 83.59(14) . . ?
O10 Nb2 O11 173.40(14) . . ?
O17 Nb2 O11 81.02(14) . . ?
O6 Nb2 O11 78.52(13) . . ?
O3 Nb2 O11 75.95(12) . . ?
O8 Nb2 O11 74.90(13) . . ?
O10 Nb2 Nb4 136.52(12) . . ?
O17 Nb2 Nb4 82.37(10) . . ?
O6 Nb2 Nb4 32.63(11) . . ?
O3 Nb2 Nb4 122.46(9) . . ?
O8 Nb2 Nb4 83.36(9) . . ?
O11 Nb2 Nb4 46.55(8) . . ?
O10 Nb2 Nb1 138.20(12) . . ?
O17 Nb2 Nb1 33.46(11) . . ?
O6 Nb2 Nb1 85.51(11) . . ?
O3 Nb2 Nb1 81.16(9) . . ?
O8 Nb2 Nb1 122.44(10) . . ?
O11 Nb2 Nb1 47.57(9) . . ?
Nb4 Nb2 Nb1 60.49(3) . . ?
O18 Nb3 O9 103.83(16) . . ?
O18 Nb3 O4 100.98(16) . . ?
O9 Nb3 O4 92.84(15) . . ?
O18 Nb3 O1 101.63(15) . . ?
O9 Nb3 O1 91.05(14) . . ?
O4 Nb3 O1 155.41(14) . . ?
O18 Nb3 O3 100.41(15) . . ?
O9 Nb3 O3 155.73(14) . . ?
O4 Nb3 O3 83.86(14) . . ?
O1 Nb3 O3 82.68(14) . . ?
O18 Nb3 O11 175.56(14) . . ?
O9 Nb3 O11 80.46(13) . . ?
O4 Nb3 O11 79.81(13) . . ?
O1 Nb3 O11 76.92(13) . . ?
O3 Nb3 O11 75.29(12) . . ?
O18 Nb3 Nb6 134.21(12) . . ?
O9 Nb3 Nb6 80.58(11) . . ?
O4 Nb3 Nb6 124.55(10) . . ?
O1 Nb3 Nb6 32.74(9) . . ?
O3 Nb3 Nb6 81.59(9) . . ?
O11 Nb3 Nb6 44.75(9) . . ?
O18 Nb3 Nb1 132.98(12) . . ?
O9 Nb3 Nb1 83.11(11) . . ?
O4 Nb3 Nb1 32.06(10) . . ?
O1 Nb3 Nb1 124.97(10) . . ?
O3 Nb3 Nb1 81.44(9) . . ?
O11 Nb3 Nb1 48.10(9) . . ?
Nb6 Nb3 Nb1 92.75(2) . . ?
O18 Nb3 Nb5 137.42(12) . . ?
O9 Nb3 Nb5 33.61(10) . . ?
O4 Nb3 Nb5 84.79(10) . . ?
O1 Nb3 Nb5 85.10(10) . . ?
O3 Nb3 Nb5 122.18(9) . . ?
O11 Nb3 Nb5 46.91(8) . . ?
Nb6 Nb3 Nb5 60.065(19) . . ?
Nb1 Nb3 Nb5 61.01(2) . . ?
O12 Nb4 O2 105.21(16) . . ?
O12 Nb4 O5 102.38(16) . . ?
O2 Nb4 O5 92.06(15) . . ?
O12 Nb4 O6 102.45(16) . . ?
O2 Nb4 O6 90.43(14) . . ?
O5 Nb4 O6 153.44(14) . . ?
O12 Nb4 O14 99.92(16) . . ?
O2 Nb4 O14 154.86(14) . . ?
O5 Nb4 O14 83.39(14) . . ?
O6 Nb4 O14 83.20(14) . . ?
O12 Nb4 O11 174.42(15) . . ?
O2 Nb4 O11 80.29(13) . . ?
O5 Nb4 O11 78.12(13) . . ?
O6 Nb4 O11 76.26(13) . . ?
O14 Nb4 O11 74.57(13) . . ?
O12 Nb4 Nb2 133.77(13) . . ?
O2 Nb4 Nb2 80.04(10) . . ?
O5 Nb4 Nb2 123.56(10) . . ?
O6 Nb4 Nb2 31.44(10) . . ?
O14 Nb4 Nb2 81.98(10) . . ?
O11 Nb4 Nb2 45.44(8) . . ?
O12 Nb4 Nb5 134.34(12) . . ?
O2 Nb4 Nb5 82.66(11) . . ?
O5 Nb4 Nb5 31.97(10) . . ?
O6 Nb4 Nb5 122.69(10) . . ?
O14 Nb4 Nb5 80.47(10) . . ?
O11 Nb4 Nb5 46.45(8) . . ?
Nb2 Nb4 Nb5 91.764(16) . . ?
O12 Nb4 Nb1 138.18(13) . . ?
O2 Nb4 Nb1 33.00(10) . . ?
O5 Nb4 Nb1 83.52(10) . . ?
O6 Nb4 Nb1 84.28(10) . . ?
O14 Nb4 Nb1 121.90(10) . . ?
O11 Nb4 Nb1 47.34(8) . . ?
Nb2 Nb4 Nb1 60.175(19) . . ?
Nb5 Nb4 Nb1 60.351(14) . . ?
O16 Nb5 O15 102.18(16) . . ?
O16 Nb5 O5 102.74(15) . . ?
O15 Nb5 O5 89.42(15) . . ?
O16 Nb5 O9 102.53(15) . . ?
O15 Nb5 O9 86.19(15) . . ?
O5 Nb5 O9 154.72(14) . . ?
O16 Nb5 O7 103.51(16) . . ?
O15 Nb5 O7 154.16(14) . . ?
O5 Nb5 O7 87.64(14) . . ?
O9 Nb5 O7 85.60(14) . . ?
O16 Nb5 O11 179.50(15) . . ?
O15 Nb5 O11 77.96(13) . . ?
O5 Nb5 O11 77.74(12) . . ?
O9 Nb5 O11 76.99(13) . . ?
O7 Nb5 O11 76.33(13) . . ?
O16 Nb5 Nb6 135.36(13) . . ?
O15 Nb5 Nb6 122.31(10) . . ?
O5 Nb5 Nb6 82.59(10) . . ?
O9 Nb5 Nb6 78.83(10) . . ?
O7 Nb5 Nb6 31.89(10) . . ?
O11 Nb5 Nb6 44.46(8) . . ?
O16 Nb5 Nb3 134.08(12) . . ?
O15 Nb5 Nb3 79.23(10) . . ?
O5 Nb5 Nb3 123.17(10) . . ?
O9 Nb5 Nb3 31.60(10) . . ?
O7 Nb5 Nb3 80.98(10) . . ?
O11 Nb5 Nb3 45.45(8) . . ?
Nb6 Nb5 Nb3 59.60(3) . . ?
O16 Nb5 Nb4 134.39(12) . . ?
O15 Nb5 Nb4 79.49(11) . . ?
O5 Nb5 Nb4 31.95(10) . . ?
O9 Nb5 Nb4 122.96(10) . . ?
O7 Nb5 Nb4 84.57(10) . . ?
O11 Nb5 Nb4 46.10(8) . . ?
Nb6 Nb5 Nb4 64.326(17) . . ?
Nb3 Nb5 Nb4 91.362(16) . . ?
O13 Nb6 O7 104.86(16) . . ?
O13 Nb6 O1 102.98(16) . . ?
O7 Nb6 O1 94.64(15) . . ?
O13 Nb6 O14 99.43(16) . . ?
O7 Nb6 O14 87.28(15) . . ?
O1 Nb6 O14 156.18(15) . . ?
O13 Nb6 O8 97.97(16) . . ?
O7 Nb6 O8 155.83(14) . . ?
O1 Nb6 O8 87.79(14) . . ?
O14 Nb6 O8 81.18(14) . . ?
O13 Nb6 O11 173.10(15) . . ?
O7 Nb6 O11 81.15(14) . . ?
O1 Nb6 O11 79.62(13) . . ?
O14 Nb6 O11 77.23(13) . . ?
O8 Nb6 O11 75.63(13) . . ?
O13 Nb6 Nb3 137.21(12) . . ?
O7 Nb6 Nb3 83.19(11) . . ?
O1 Nb6 Nb3 34.29(10) . . ?
O14 Nb6 Nb3 123.13(10) . . ?
O8 Nb6 Nb3 85.46(10) . . ?
O11 Nb6 Nb3 45.92(8) . . ?
O13 Nb6 Nb5 138.91(12) . . ?
O7 Nb6 Nb5 34.08(11) . . ?
O1 Nb6 Nb5 86.58(11) . . ?
O14 Nb6 Nb5 81.77(10) . . ?
O8 Nb6 Nb5 122.52(9) . . ?
O11 Nb6 Nb5 47.10(8) . . ?
Nb3 Nb6 Nb5 60.33(2) . . ?
O16 Na1 O4W 107.74(19) . . ?
O16 Na1 O10 104.14(17) . 2_546 ?
O4W Na1 O10 107.16(18) . 2_546 ?
O16 Na1 O2W 95.77(17) . . ?
O4W Na1 O2W 140.8(2) . . ?
O10 Na1 O2W 96.44(17) 2_546 . ?
O12 Na2 O7W 126.1(2) . . ?
O12 Na2 O6W 116.7(2) . 3_656 ?
O7W Na2 O6W 93.78(18) . 3_656 ?
O12 Na2 N7 68.17(15) . 2_556 ?
O7W Na2 N7 113.6(2) . 2_556 ?
O6W Na2 N7 142.3(2) 3_656 2_556 ?
O19 Na3 O4W 95.65(19) . 3_657 ?
O19 Na3 O3W 101.12(19) . 2_556 ?
O4W Na3 O3W 114.8(2) 3_657 2_556 ?
O19 Na3 O9W 100.4(2) . 3_557 ?
O4W Na3 O9W 93.34(19) 3_657 3_557 ?
O3W Na3 O9W 142.3(2) 2_556 3_557 ?
Nb6 O1 Nb3 112.97(16) . . ?
Nb4 O2 Nb1 116.11(17) . . ?
Nb2 O3 Nb3 112.10(14) . . ?
Nb3 O4 Nb1 116.18(17) . . ?
Nb5 O5 Nb4 116.08(16) . . ?
Nb2 O6 Nb4 115.93(18) . . ?
Nb6 O7 Nb5 114.03(18) . . ?
Nb2 O8 Nb6 111.96(15) . . ?
Nb3 O9 Nb5 114.79(17) . . ?
Nb3 O9 Cu3 122.46(16) . . ?
Nb5 O9 Cu3 121.90(15) . . ?
Nb2 O10 Na1 121.22(19) . 2_556 ?
Nb6 O11 Nb2 97.46(13) . . ?
Nb6 O11 Nb3 89.33(12) . . ?
Nb2 O11 Nb3 96.24(12) . . ?
Nb6 O11 Nb4 96.93(13) . . ?
Nb2 O11 Nb4 88.01(12) . . ?
Nb3 O11 Nb4 171.93(16) . . ?
Nb6 O11 Nb5 88.44(12) . . ?
Nb2 O11 Nb5 172.95(16) . . ?
Nb3 O11 Nb5 87.65(12) . . ?
Nb4 O11 Nb5 87.44(11) . . ?
Nb6 O11 Nb1 173.83(17) . . ?
Nb2 O11 Nb1 87.50(12) . . ?
Nb3 O11 Nb1 86.48(11) . . ?
Nb4 O11 Nb1 86.86(11) . . ?
Nb5 O11 Nb1 86.87(11) . . ?
Nb4 O12 Na2 152.3(2) . . ?
Nb6 O13 Cu2 163.7(2) . . ?
Nb6 O14 Nb4 111.04(16) . . ?
Nb5 O15 Nb1 118.48(17) . . ?
Nb5 O16 Na1 163.0(2) . . ?
Nb2 O17 Nb1 115.41(17) . . ?
Nb1 O19 Na3 157.3(3) . . ?
Na1 O4W Na3 141.2(2) . 3_657 ?
N9 C1 C6 107.6(4) . . ?
N3 C2 C7 107.9(5) . . ?
N5 C3 C8 107.7(5) . . ?
N2 C4 C5 107.3(5) . . ?
N4 C5 C4 107.6(5) . . ?
N8 C6 C1 109.5(4) . . ?
N10 C7 C2 108.1(5) . . ?
N7 C8 C3 107.7(5) . . ?
N6 C9 C10 108.8(5) . . ?
N1 C10 C9 108.8(5) . . ?
C10 N1 Cu2 109.8(3) . . ?
C4 N2 Cu2 106.3(3) . . ?
C2 N3 Cu1 108.2(3) . . ?
C5 N4 Cu2 110.4(3) . . ?
C3 N5 Cu3 108.2(3) . . ?
C9 N6 Cu2 108.2(4) . . ?
C8 N7 Cu3 109.1(3) . . ?
C8 N7 Na2 116.4(4) . 2_546 ?
Cu3 N7 Na2 100.4(2) . 2_546 ?
C6 N8 Cu3 111.2(3) . . ?
C1 N9 Cu3 105.6(3) . . ?
C7 N10 Cu1 108.2(3) . . ?
N3 Cu1 N3 180.0 3_657 . ?
N3 Cu1 N10 85.16(18) 3_657 3_657 ?
N3 Cu1 N10 94.84(18) . 3_657 ?
N3 Cu1 N10 94.84(18) 3_657 . ?
N3 Cu1 N10 85.16(18) . . ?
N10 Cu1 N10 180.000(1) 3_657 . ?
N2 Cu2 N1 174.8(2) . . ?
N2 Cu2 N4 84.20(19) . . ?
N1 Cu2 N4 95.88(19) . . ?
N2 Cu2 N6 94.1(2) . . ?
N1 Cu2 N6 85.1(2) . . ?
N4 Cu2 N6 172.2(2) . . ?
N2 Cu2 O13 95.72(17) . . ?
N1 Cu2 O13 89.52(17) . . ?
N4 Cu2 O13 91.43(17) . . ?
N6 Cu2 O13 96.36(18) . . ?
N5 Cu3 N9 178.52(19) . . ?
N5 Cu3 N8 94.69(19) . . ?
N9 Cu3 N8 84.19(18) . . ?
N5 Cu3 N7 84.65(19) . . ?
N9 Cu3 N7 96.32(19) . . ?
N8 Cu3 N7 171.66(19) . . ?
N5 Cu3 O9 90.27(16) . . ?
N9 Cu3 O9 90.75(16) . . ?
N8 Cu3 O9 92.69(16) . . ?
N7 Cu3 O9 95.62(16) . . ?
_diffrn_measured_fraction_theta_max 0.995
_diffrn_reflns_theta_full        27.48
_diffrn_measured_fraction_theta_full 0.995
_refine_diff_density_max         1.164
_refine_diff_density_min         -1.180
_refine_diff_density_rms         0.171